CN105670037A - Surface treatment method of nanometer calcium carbonate for flame-retardant PVC wood-plastic composite - Google Patents
Surface treatment method of nanometer calcium carbonate for flame-retardant PVC wood-plastic composite Download PDFInfo
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Abstract
The invention discloses a surface treatment method of nanometer calcium carbonate for a flame-retardant PVC wood-plastic composite. The surface treatment method of nanometer calcium carbonate comprises the following steps: heating a nanometer calcium carbonate slurry to 50-70 DEG C, in which the pH value is 6.5-7.5, the specific area is 18-25 m<2>/g and the mass concentration is 13-16%, and then keeping constant temperature; adding a betaine-phosphate composite surfactant to the suspension, continuing to stir for 30-60 minutes to obtain a modified slurry; respectively carrying out pressure filtration to dehydrate, drying, crushing and grading to the modified slurry according to a regular method, so as to obtain the nanometer calcium carbonate product. According to the surface treatment method disclosed by the invention, betaine and phosphate are composited to prepare the surfactant; the treated nanometer calcium carbonate product is good in dispersion, well compatible with PVC resin and wood powder, capable of being filled at high volume, further capable of enabling the wood-plastic composite to achieve a better processing property and improve the mechanical property of the composite, good in flame retardance, and capable of beautifying the product appearance.
Description
Technical field
The invention belongs to technical field of nano material, relate to the surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate.
Background technology
PVC wood plastic composite material has the advantage of timber and plastics concurrently, such as good stability of the dimension, corrosion-resistant, resistance to damages by worms, easy machine-shaping, and recoverable. Wood plastic composite in North America especially the U.S. have become as strong industry. They are just being used in various new occasion, such as cover plate, harbour, landscape material, enclosure wall, marker post, flooring block, railroad tie, sports ground apparatus, door window frame, building, molded automotive interior instrument etc. But its application has the right requirement of resistance mostly, therefore give the needs that the good fire resistance of wood plastic composite is this kind of Materials. The current most polarity of wood and plastic composite material flame-retardant is relatively strong, poor with the polymer body compatibility, when addition is few, does not reach fire-retardant effect. When these fire retardant additions are big, it is easy to produce space with basal body interface, reduce the mechanical property of wood plastic composite.
Chinese patent CN101143952A discloses the flame resistant method of a kind of Intumscent Flame Retardant System added in Polyvinyl chloride wood-plastic composite material and polystyrene wood plastic composite respectively based on APP. The addition of APP can increase the limited oxygen index of wood plastic composite effectively, reduces HRR, but its addition causes that greatly material mechanical performance declines to a great extent.
Chinese patent CN105111614A discloses the PVC wood plastic material preparation method that a kind of asepsis environment-protecting is fire-retardant, and the method reaches certain fire retardation by adding Kaolin, but its limited efficiency.
Nano-calcium carbonate is as a kind of new type functional inorganic material, by wide shipping for industries such as rubber, plastics, coating, fluid sealant, ink and papermaking. Owing to nano-calcium carbonate particle diameter is little, specific surface energy is high, after surface modification, make it have the unexistent surface activity of general inorganic filler, be widely used in PVC wood plastic composite material in recent years.But the nano-calcium carbonate of long time without surface modification is difficult to be dispersed in composite, not only do not play effect of nano material, the mechanical property of goods can be reduced on the contrary. At present in nono calcium carbonate modified method, the main surface conditioning agent selected is generally fatty acid or its salt. But the compatibility of PVC wood plastic composite material and fatty acid or soap is poor, it is difficult to effectively be combined with nano-calcium carbonate filler, causes that the interfacial adhesion of matrix and filler is poor, thus causing the mechanical strength of composite not high.
Therefore, find and a kind of can give PVC wood plastic material excellent flame retardancy and make the nano-calcium carbonate filler of its mechanical property keeping it good be particularly important.
Summary of the invention
The present invention is directed to existing nono calcium carbonate modified Problems existing, it is provided that the surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate. Nano-calcium carbonate is carried out surface modification by adopting glycine betaine and phosphate ester by the method, nano-calcium carbonate is made to have the good compatibility and dispersibility in the composite, improve the interfacial adhesion of polyvinyl chloride resin and wood fibre, to also having good fire retardation while PVC wood plastic composite material activeness and quietness.
The present invention is based on following principle and realizes:
This programme adopts Phosphate Anionic Surfactants and beet alkali ampholytic surface active agent that nano-calcium carbonate is carried out surface modification. There is due to beet alkali surface activator excellent dissolubility and compatibility, composite with phosphate ester surfactants improve surface treatment effect. Glycine betaine is alkaloid, and wood fibre is many in acidity, and the nano-calcium carbonate after glycine betaine process has the good compatibility with wood fibre. Phosphate ester is a kind of nano-calcium carbonate surface conditioning agent, also it is the conventional fire retardant of PVC wood plastic composite material, it is coated on nano-calcium carbonate surface by composite with glycine betaine, make it have P-N cooperative effect, adding nano-calcium carbonate a large amount in PVC wood plastic composite material to fill, flame retardant effect is more notable.
For realizing object above, the technical solution used in the present invention is as follows:
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 18～25m by pH=6.5～7.5, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 13～16%, and heating, to 50～70 DEG C, keeps constant temperature;
(2) adding glycine betaine and phosphate ester compound base amount method agent again to the suspension slurry of step (1), continuously stirred 30～60min must modifiy serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
Preferably, the above nano-calcium carbonate serosity is cubic in class by chemical precipitation method preparation. Concrete preparation method: choose the calcium carbonate content limestone more than 98% and calcine 3 hours at 1100 DEG C and obtain quick lime. Quick lime and 60 ± 5 DEG C of water carry out fully digestion by weight 1:5 and obtain slaked lime slurry. Slaked lime slurry is sieved after slagging-off, add tap water, be diluted to mass concentration 9.5～12.5%, and be refrigerated to 18～22 DEG C. Pass into purification, cooling after CO2Lime white after the lime-kiln gas of volumetric concentration 30～35% and process carries out carbonation reaction, and when reacting liquid pH value, < when 7.5, carbonation reaction completes, and prepares required nano-calcium carbonate suspension slurry.
Preferably, in the above compound base amount method agent, the mass ratio of glycine betaine and phosphate ester is 1～6:1.
Preferably, the above to be the addition of glycine betaine and phosphate ester be in suspension slurry the 1.5～3.2% of calcium carbonate dry substrate amount.
Preferably, the above compound base amount method agent preparation method is as follows: add phosphate ester in 50～70 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 2～5min.
Compared with prior art, beneficial effects of the present invention:
1, the nano-calcium carbonate calcium product good dispersion that prepared by the present invention, the good compatibility is had with polyvinyl chloride resin and wood powder, a large amount filling can be carried out, can also give wood plastic composite good processing characteristics, improve composite materials property, there is better flame retardant effect, beautify products appearance, play functional modification effect.
2, the inventive method adopt phosphate ester and glycine betaine are re-dubbed surface conditioning agent, phosphate ester is a kind of surface conditioning agent, also it is the conventional fire retardant of PVC wood plastic composite material, it is coated on nano-calcium carbonate surface by composite with glycine betaine, make it have P-N cooperative effect, adding nano-calcium carbonate a large amount in PVC wood plastic composite material to fill, flame retardant effect is more notable.
3, the present invention is using phosphate ester as surface conditioning agent, eliminates interpolation fire retardant mix homogeneously step, simplifies technological process, improve production efficiency in the preparation process of wood plastic composite.
4, the inventive method is raw materials used cheap and easy to get, technique simple possible, it is easy to realize industrialized production, has good economic benefit and social benefit.
Detailed description of the invention
Below in conjunction with specific embodiment to the detailed description of the invention, but it is not limited to protection scope of the present invention.
Embodiment 1
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 18.2m by pH=6.8, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 15%, and heating, to 50 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 2.5% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 4:1, and continuously stirred 30min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 120 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 50 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 2min.
Embodiment 2
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 17.9m by pH=6.8, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 13%, and heating, to 70 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 1.8% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 4:1, and continuously stirred 45min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 110 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 70 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 3min.
Embodiment 3
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 25.2m by pH=7.0, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 13%, and heating, to 60 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 3.2% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 4:1, and continuously stirred 60min obtains modified serosity;
It is (3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry at 130 DEG C, pulverize, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 60 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 5min.
Embodiment 4
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 22.3m by pH=7.1, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 13.5%, and heating, to 50 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 2.5% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 6:1, and continuously stirred 40min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 120 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 50 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 5min.
Embodiment 5
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 19.2m by pH=6.5, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 16%, and heating, to 65 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 1.5% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 5:1, and continuously stirred 30min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 100 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 65 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 2min.
Embodiment 6
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 23.6m by pH=7.5, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 15%, and heating, to 55 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 3.0% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 1:1, and continuously stirred 30min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 110 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 55 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 3min.
Embodiment 7
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 21.3m by pH=7.2, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 14%, and heating, to 60 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 3.2% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 2:1, and continuously stirred 60min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 130 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 60 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 5min.
Embodiment 8
The surface treatment method of a kind of flame retardant type PVC wood plastic composite material nano-calcium carbonate, comprises the following steps:
(1) it is 18.6m by pH=7.0, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 15%, and heating, to 50 DEG C, keeps constant temperature;
(2) glycine betaine and phosphate ester compound base amount method agent are added again to the suspension slurry of step (1), wherein the addition of glycine betaine and phosphate ester is the 2.5% of calcium carbonate dry substrate amount, the mass ratio of glycine betaine and phosphate ester is 3:1, and continuously stirred 45min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 120 DEG C, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
The preparation method of described compound base amount method agent is as follows: add phosphate ester in 50 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, adds glycine betaine, stir, obtain compound base amount method agent after stirring 5min.
Comparative example 1
(1) it is 18.6m by pH=7.0, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 15%, and heating, to 50 DEG C, keeps constant temperature;
(2) adding stearic acid saponification liquor inorganic agent to the suspension slurry of step (1) again, wherein stearic acid addition is the 2.5% of calcium carbonate dry substrate amount, and continuously stirred 45min obtains modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize at 120 DEG C, classification, obtain nano-calcium carbonate calcium product.
Being prepared by stearic acid and sodium hydroxide in temperature of described stearic acid saponification liquor inorganic agent is carry out saponification in 90 DEG C of tap waters, and wherein the consumption of sodium hydroxide is the 15% of stearic acid quality, and stearic acid saponification liquor mass concentration is 10%.
Comparative example 2
(1) it is 18.6m by pH=7.0, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 15%, and heating, to 50 DEG C, keeps constant temperature;
(2) adding phosphate ester surface conditioning agent to the suspension slurry of step (1) again, wherein the addition of phosphate ester is the 2.5% of calcium carbonate dry substrate amount, and continuously stirred 45min obtains modified serosity;
(3) by modified serosity obtained above respectively through filter-press dehydration, dry, pulverize at 120 DEG C, classification, obtain nano-calcium carbonate calcium product.
The preparation method of described phosphate ester surface conditioning agent is as follows: adds phosphate ester in 50 DEG C of hot water, is configured to the phosphate ester solution that mass concentration is 10%, stirs 5min.
Comparative example 3
(1) it is 18.6m by pH=7.0, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 15%, and heating, to 50 DEG C, keeps constant temperature;
(2) adding glycine betaine surface conditioning agent to the suspension slurry of step (1) again, wherein the addition of glycine betaine is the 2.5% of calcium carbonate dry substrate amount, and continuously stirred 45min obtains modified serosity;
(3) by modified serosity obtained above respectively through filter-press dehydration, dry, pulverize at 120 DEG C, classification, obtain nano-calcium carbonate calcium product.
The nano-calcium carbonate calcium product that above-described embodiment and comparative example obtain is made PVC wood plastic composite material goods by the formula of table 1. After making composite, carry out performance test by working standard, wherein fire resistance test result in Table 2, mechanical experimental results in Table 3.
Table 1:PVC wood plastic composite formula table
| Raw material | Number |
| PVC | 100 |
| Wood powder | 30 |
| Nano-calcium carbonate | 45 |
| Hlf-2 calcium-zinc composite stabilizing agent | 11 |
| ACR-401 processing aid | 6 |
| ACR-530 foaming control agent | 6 |
| Foaming agent | 1.4 |
| Lubricant | 1.8 |
Table 2: each embodiment and comparative example make the fire resistance test result of PVC wood plastic composite material
From the flame retardant test result of table 2 it can be seen that nano-calcium carbonate prepared by the present invention is applied to preparation PVC wood plastic composite material, compared with comparative example, flame-retardant smoke inhibition effect is notable.
Table 3: each embodiment and comparative example make the mechanical experimental results of PVC wood plastic composite material
Can be seen that from the mechanical experimental results of table 3, after adopting phosphate ester and glycine betaine composite surface conditioning agent that nano-calcium carbonate is modified, compared with single phosphate ester, glycine betaine or stearic acid salt, nano-calcium carbonate and wood plastic composite have the good compatibility and interfacial adhesion so that it is the PVC wood plastic composite material after filling has more excellent mechanical property.
Claims (4)
1. the surface treatment method of a flame retardant type PVC wood plastic composite material nano-calcium carbonate, it is characterised in that: comprise the following steps:
(1) it is 18～25m by pH=6.5～7.5, specific surface area2/ g, mass concentration are the nano-calcium carbonate suspension slurry of 13～16%, heat to 50～70 DEG C, constant temperature;
(2) add glycine betaine and phosphate ester compound base amount method agent, continuously stirred 30～60min again to the suspension slurry of step (1), obtain modified serosity;
(3) by modified serosity obtained above according to a conventional method respectively through filter-press dehydration, dry, pulverize, classification, obtain PVC wood plastic composite material nano-calcium carbonate calcium product.
2. the surface treatment method of flame retardant type PVC wood plastic composite material nano-calcium carbonate according to claim 1, it is characterised in that: in described compound base amount method agent, the mass ratio of glycine betaine and phosphate ester is 1～6:1.
3. the surface treatment method of flame retardant type PVC wood plastic composite material nano-calcium carbonate according to claim 1, it is characterised in that: the addition of described glycine betaine and phosphate ester is in suspension slurry the 1.5～3.2% of calcium carbonate dry substrate amount.
4. the surface treatment method of flame retardant type PVC wood plastic composite material nano-calcium carbonate according to claim 1, it is characterized in that: described compound base amount method agent preparation method is as follows: in 50～70 DEG C of hot water, add phosphate ester, it is configured to the phosphate ester solution that mass concentration is 10%, in solution, glycine betaine is added again after stirring 2～5min, stir, obtain compound base amount method agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109232986A (en) * | 2018-07-12 | 2019-01-18 | 广西合山市华纳新材料科技有限公司 | A kind of preparation method of PVC cable special-purpose anti-flaming calcium carbonate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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